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14 protocols using q500 analyzer

1

Organic Synthesis and Characterization

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All air and water sensitive reactions were performed under a nitrogen atmosphere. Tetrahydrofuran and toluene were dried over Na/benzophenone ketyl and were freshly distilled prior to use. The other materials were of the common commercial level and were used as received. Thin layer chromatography (TLC) was conducted on flexible sheets precoated with SiO2 and the separated products were visualized by UV light. Column chromatography was conducted using SiO2 (300 mesh) from Fisher Scientific. 1H and 13C NMR spectra were recorded on a Bruker ARX-400 (400 MHz) or ARX-500 (500 MHz) spectrometer, using CDCl3. All chemical shifts were reported in parts per million (ppm). The 1H NMR chemical shifts were referenced to TMS (0 ppm), and the 13C NMR chemical shifts were referenced to CDCl3 (77.23 ppm). HR-ESI-MS data were recorded on a Bruker APEX IV mass spectrometer. Thermal gravimetric analysis (TGA) was carried out on a TA Instrument Q500 analyzer. Absorption spectra were recorded on a PerkinElmer Lambda 750 UV-vis spectrometer. Photoluminescence was recorded on a Perkin-Elmer LS 55 spectrofluorometer and a HORIBA JobinYvon Nanolog FL3-2iHR spectrometer.
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2

Thermal Analysis of Polymer Samples

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Thermogravimetric analysis
(TGA) of the polymer samples was carried out in platinum pans using
a TA Instruments Q500 analyzer under N2 flow from room
temperature to 600 °C at a ramp rate of 10 °C/min. Differential
scanning calorimetry (DSC) was carried out using a TA Instruments
Q200 calorimeter between −50 and 200 °C. For both TGA
and DSC measurements, sample weights were between 1.5 and 8 mg.
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3

Thermal Analysis of Polymeric Nanoparticles

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Thermogravimetric analysis (TGA) was carried out to determine the percentage of each component (namely, P(VDF-TrFE) and DSPE-PEG) in plain PNPs with a Q500 analyzer (TA Instrument), by heating the samples from 30 to 700°C at a heating rate of 5°C/min under nitrogen atmosphere (flow rate of 50 mL/min).
Differential scanning calorimetry (DSC) curves were obtained using a DSC-1 STARe System (Mettler Toledo) to obtain information regarding the thermal behavior of P(VDF-TrFE), DSPE-PEG, and plain PNPs. The DSC analysis has been performed on 1 mg of freeze-dried samples from 20 to 200°C at a heating rate of 10°C/min. The reported thermograms represent the first heating ramp to portray the crystallinity of the obtained nanoparticles, avoiding the reorganization in bigger aggregates due to the melting phenomenon that could result into the second heating ramp.
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4

Characterization of Composite Materials

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The composites' morphologies were characterized by scanning electron microscopy (SEM) using a JSM6510 microscope (JEOL) using the secondary electron mode. Thermal analysis was conducted at the range of 25 °C to 600 °C using a Q500 analyzer (TA Instruments, New Castle, DE, USA) with a heating rate of 10 °C min−1 under nitrogen atmosphere. For the differential scanning calorimetry (DSC), samples were heated from 25 to 250 °C in a DSC Q100 (TA Instruments, USA) under nitrogen atmosphere. Fourier Transform Infrared was carried out in an FTIR spectrophotometer VERTEX 70 (Bruker Corporation) with ATR technique. Proton and carbon nuclear magnetic resonance (1H- and 13C- NMR) spectra were obtained on a 600 MHz Avance III HD Bruker spectrometer using dimethyl sulfoxide (DMSO-d6) as a solvent and tetramethylsilane (TMS) as the internal reference.
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5

Mechanical and Thermal Characterization of Lignin-based Bioplastics

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The
mechanical properties of samples were characterized by uniaxial tensile
tests on a dual column Instron 3365 universal testing machine equipped
with a 500 N load cell. The tensile measurements were conducted according
to ASTM D 882 Standard Test Methods for Tensile Properties of Thin
Plastic Sheeting. For this, dog-bone shaped samples (25 mm length,
4 mm width) were stretched at a rate of 2 mm/min. Stress–strain
curves were recorded at 25 °C and 44% relative humidity (RH).
A minimum of seven measurements was carried out for each sample, and
the results were averaged to obtain a mean value. The values of Young’s
modulus, toughness (taken as the area below the curve, i.e., the fracture
energy), stress, and elongation at break were calculated from the
stress–strain curves.
The thermal degradation behavior
of lignin-based bioplastic samples was investigated through thermogravimetric
analysis (TGA) using a Q500 analyzer from TA Instruments. The measurements
were carried out under an inert N2 atmosphere on 3 mg samples
in an aluminum pan at a heating rate of 10 °C/min, from 30 to
600 °C. The weight loss (TG curve) and its first derivative (DTG
curve) were recorded simultaneously as a function of time and temperature.
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6

Thermogravimetric Analysis of Small Samples

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TGA was performed on small samples (5 mg) using a Q500 analyzer from TA Instruments. The scans were performed in the range of 30–600 °C, using a 10 °C min–1 heating rate. Cooling was achieved using 50 ml min–1 nitrogen flow.
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7

Comprehensive Material Characterization by Advanced Techniques

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SEM and EDS analyses were performed on a JSM-IT500HR scanning electron microscope (JEOL, Tokyo, Japan) equipped with an Xplore EDS detector (Oxford Instruments, Abingdon, UK) with acceleration voltages ranging from 5 to 10 kV. The materials were coated with platinum prior to SEM observation. PXRD patterns were obtained using a SmartLab diffractometer (Rigaku, Tokyo, Japan). ATR-FTIR spectra were acquired using a Nicolet iS50 spectrometer (Thermo Fisher Scientific, Waltham, MA, USA). TGA measurements were performed using a Q500 analyzer (TA Instruments, New Castle, PA, USA) by heating the sample from 30 to 800 °C at a rate of 10 °C/min under nitrogen gas. DVS measurements were performed at 25 °C using a DVS Intrinsic analyzer (Surface Measurement Systems, London, UK). Nitrogen adsorption measurements were performed at 77 K using an ASAP 2020 system (Micromeritics Instrument Corp., Norcross, GA, USA). Before analysis, the samples were degassed at 393 K for 2 h under vacuum. The nitrogen isotherm data were used to calculate the specific surface area using the BET method and the pore size distribution using a DFT model.
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8

Thermal Analysis of Samples

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TGA analysis of the samples was carried out on a TA instrument Q500 analyzer both under nitrogen and air atmosphere with a 40 ml/min flow in a dynamic non-isothermal mode at a heating rate of 20 °C/min from ambient temperature to 700 °C.
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9

Comprehensive Material Characterization Protocol

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PXRD data were collected on a Rigaku Ultima IV diffractometer with Cu Kα radiation (λ = 1.5418 Å). The TEM and HRTEM images were taken on an FEI Tecnai G2 S-Twin F20 TEM and FEI Titan G2 60-300 scanning TEM. The infrared absorption spectra were recorded on a Bruker FTIR IFS-66V/S spectrometer in the range of 400 to 4000 cm−1 with KBr pellets. A baseline correction was applied after measurement. UV-vis adsorption spectra were recorded on a Shimadzu UV-2550 spectrophotometer. The XPS measurements were performed using a Thermo ESCALAB 250 spectrometer with monochromatized Al Kα excitation. LC-HRMS was performed on a high-performance liquid chromatography (Agilent 1290) and HRMS (microTOF-Q II, Bruker Daltonics)]. Thermogravimetric (TG) analysis was performed on a TA Q500 analyzer in air from room temperature to 800°C at 5°C/min. CHN analysis was conducted on a PerkinElmer 2400 elemental analyzer.
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10

Fiber Morphology and Drug Encapsulation Analysis

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The fiber morphology was observed using a Leica Cambridge Stereoscan 360 Scanning Electron Microscope (SEM) operating at 20 kV. The samples were sputter-coated with gold prior to examination.
The fiber diameter distribution of each scaffold was determined by measuring 100 fibers, and the results are given as the average diameter ± standard deviation.
The encapsulation efficiency (EE) was calculated by the following equation: EE (%)=Actual drug amountTheoretical drug amount×100
where the Actual drug amount was determined by the assay methods reported in Section 2.2.3 andSection 2.2.4.
Thermogravimetric analyses (TGA) were carried out using a TA Instruments (New Castle, DE, USA) Q500 Analyzer. Samples were heated at a rate of 10 °C min−1 from RT to 700 °C, under nitrogen flow. Differential scanning calorimetry (DSC) was carried out with a TA Instruments DSC Q2000 equipped with a refrigerated cooling system (RCS). The samples were subjected to a first heating scan at 20 °C min−1 from −90 °C to 200 °C, followed by quenching, and a second heating scan at 20 °C min−1.
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